Method for preparing samples for imaging

ABSTRACT

A method and apparatus is provided for preparing samples for observation in a charged particle beam system in a manner that reduces or prevents artifacts. Material is deposited onto the sample using charged particle beam deposition just before or during the final milling, which results in an artifact-free surface. Embodiments are useful for preparing cross sections for SEM observation of samples having layers of materials of different hardnesses. Embodiments are useful for preparation of thin TEM samples.

This application is a continuation-in-part of U.S. patent applicationSer. No. 14/081,947, filed Nov. 15, 2013, which claims priority fromU.S. Prov. Pat. App. 61/747,512, filed Dec. 31, 2012, and is acontinuation-in-part of U.S. patent application Ser. No. 13/481,351,filed May 25, 2012, which claims priority from U.S. Prov. App. No.61/493,308, filed Jun. 3, 2011, all of which are hereby incorporated byreference.

TECHNICAL FIELD OF THE INVENTION

The present invention relates to preparation of samples for electronmicroscopy and, in particular, to preparation of high quality samples ofsemiconductors and other materials.

BACKGROUND OF THE INVENTION

Semiconductor manufacturing, such as the fabrication of integratedcircuits, typically entails the use of photolithography. A semiconductorsubstrate on which circuits are being formed, usually a silicon wafer,is coated with a material, such as a photoresist, that changessolubility when exposed to radiation. A lithography tool, such as a maskor reticle, positioned between the radiation source and thesemiconductor substrate casts a shadow to control which areas of thesubstrate are exposed to the radiation. After the exposure, thephotoresist is removed from either the exposed or the unexposed areas,leaving a patterned layer of photoresist on the wafer that protectsparts of the wafer during a subsequent etching or diffusion process.

The photolithography process allows multiple integrated circuit devicesor electromechanical devices, often referred to as “chips,” to be formedon each wafer. The wafer is then cut up into individual dies, eachincluding a single integrated circuit device or electromechanicaldevice. Ultimately, these dies are subjected to additional operationsand packaged into individual integrated circuit chips orelectromechanical devices.

During the manufacturing process, variations in exposure and focusnecessitates that the patterns developed by lithographic processes becontinually monitored or measured to determine if the dimensions of thepatterns are within acceptable ranges. The importance of suchmonitoring, often referred to as process control, increases considerablyas pattern sizes become smaller, especially as minimum feature sizesapproach the limits of resolution available by the lithographic process.In order to achieve ever-higher device density, smaller and smallerfeature sizes are required. This may include the width and spacing ofinterconnecting lines, spacing and diameter of contact holes, and thesurface geometry such as corners and edges of various features. Featureson the wafer are three-dimensional structures and a completecharacterization must describe not just a surface dimension, such as thetop width of a line or trench, but a complete three-dimensional profileof the feature. Process engineers must be able to accurately measure thecritical dimensions (CD) of such surface features to fine tune thefabrication process and assure a desired device geometry is obtained.

Typically, CD measurements are made using instruments such as a scanningelectron microscope (SEM). In a scanning electron microscope (SEM), aprimary electron beam is focused to a fine spot that scans the surfaceto be observed. Secondary electrons are emitted from the surface as itis impacted by the primary beam. The secondary electrons are detected,and an image is formed, with the brightness at each point of the imagebeing determined by the number of secondary electrons detected when thebeam impacts a corresponding spot on the surface.

A focused ion beam (FIB) system is often used to expose a portion of asample for observation. For example, the FIB can be used to mill atrench in a circuit to expose a vertical sidewall that displays a crosssection showing the layers of the sample, such as a circuit or otherstructure having microscopic features.

As features continue to get smaller and smaller, however, there comes apoint where the features to be measured are too small for the resolutionprovided by an ordinary SEM. Transmission electron microscopes (TEMs)allow observers to see extremely small features, on the order ofnanometers. In contrast to SEMs, which only image the surface of amaterial, TEM also allows analysis of the internal structure of asample. In a TEM, a broad beam impacts the sample and electrons that aretransmitted through the sample are focused to form an image of thesample. The sample must be sufficiently thin to allow many of theelectrons in the primary beam to travel though the sample and exit onthe opposite site. Samples are typically less than 100 nm thick.

In a scanning transmission electron microscope (STEM), a primaryelectron beam is focused to a fine spot, and the spot is scanned acrossthe sample surface. Electrons that are transmitted through the substrateare collected by an electron detector on the far side of the sample, andthe intensity of each point on the image corresponds to the number ofelectrons collected as the primary beam impacts a corresponding point onthe surface.

As semiconductor geometries continue to shrink, manufacturersincreasingly rely on transmission electron microscopes (TEMs) formonitoring the process, analyzing defects, and investigating interfacelayer morphology. The term “TEM” as used herein refers to a TEM or aSTEM, and references to preparing a sample for a TEM are to beunderstood to also include preparing a sample for viewing on an STEM.

Thin TEM samples cut from a bulk sample material are known as“lamellae.” Lamellae are typically less than 100 nm thick, but for someapplications a lamella must be considerably thinner. With advancedsemiconductor fabrication processes at 30 nm and below, a lamella needsto be less than 20 nm in thickness in order to avoid overlap amongsmall-scale structures. Currently thinning below 60 nm is difficult andnot robust. Thickness variations in the sample result in lamellabending, over-milling, or other catastrophic defects. For such thinsamples, lamella preparation is a critical step in TEM analysis thatsignificantly determines the quality of structural characterization andanalysis of the smallest and most critical structures.

The use of focused ion beam (FIB) systems to create lamellae for TEMmicroscopy is known in the art. FIB systems are capable of millinglamellae sufficiently thin to be used in a TEM system. The use ofdual-beam systems for TEM sample preparation is known in the art. Adual-beam system has a FIB column for milling a lamella from a bulksample and a SEM column for imaging the lamella, typically as thelamella is being milled. Dual-beam systems improve the time required toprepare samples for TEM analysis. While the use of FIB methods in samplepreparation has reduced the time required to prepare samples for TEManalysis down to only a few hours, it is not unusual to analyze 15 to 50TEM samples from a given wafer. As a result, speed of sample preparationis a very important factor in the use of TEM analysis, especially forsemiconductor process control.

FIGS. 1A and 1B show the preparation of a sample lamella for TEManalysis from a bulk sample material using a FIB. Bulk sample material108 is loaded into sample stage and oriented so that its top surface isperpendicular to focused ion beam 104 emitted from a FIB column. Afocused ion beam using a high beam current with a correspondingly largebeam size is used to mill large amounts of material away from the frontand back portion of the region of interest. The remaining materialbetween the two milled rectangles 14 and 15 forms a thin vertical samplesection 102 that includes an area of interest. After bulk thinning, thesample section is thinned (typically using progressively finer beamsizes and lower beam energy) until the desired thickness (typically lessthan 100 nm) is reached. Most of the ion beam machining done to createlamella 110 is performed with bulk sample material 108 and FIB column inthis orientation.

Once the specimen reaches a desired thickness, the stage is typicallytilted and a U-shaped cut is made at an angle partially along the bottomand sides of the sample section 102, leaving the sample hanging by tabsat either side at the top of the sample. The small tabs allow the leastamount of material to be milled free after the sample is completely FIBpolished, reducing the possibility of redeposition artifactsaccumulating on the thin specimen. The sample section is then furtherthinned using progressively finer beam sizes. Finally, the tabs are cutto completely free the thinned lamella 110. After thinning the sample isfreed from the bulk material at the sides and bottom, and the thinnedTEM sample can be extracted.

Unfortunately, ultra thin lamellae formed using the prior art methodsdescribed above are subject to undesirable side effects known as“bending” and “curtaining.” When attempting to produce ultra thinsamples (for example, 30 nm thickness or less) the sample may losestructural integrity and deform under forces acting on the sample,typically by bending or bowing toward one sample face or the other. Ifthis occurs during or prior to a FIB thinning step, then the deformationof the region of interest toward or away from the beam may causeunacceptable damage to the sample.

Thickness variations caused by a milling artifact known as “curtaining”can also have a significant effect on TEM sample quality. When bulksample material 108 is formed from a heterogeneous structure (e.g.,metal gates and shields along with silicon and silicon dioxide), ionbeam 104 preferentially mills the lighter elements at a higher millrate. The heavier metal elements tend to shadow the lighter materialunderneath them. The resulting effect is a rippled face, which is notmilled back as far in the areas of metal as it is milled in the areaswithout metal. FIG. 2 is a photomicrograph of a thinned TEM sample 102showing curtaining on one sample face, in which the rippled features onthe lamella face resemble a hanging curtain. Curtaining artifacts reducethe quality of the TEM imaging and limit the minimal useful specimenthickness. For ultra-thin TEM samples, the two cross-section faces arein very close proximity so thickness variations from curtaining effectscan cause a sample lamella to be unusable. Thus, it is desirable toreduce curtaining artifacts during the preparation of TEM samplelamellae.

Curtaining and other artifact are also problems on cross section facesmilled by a FIB for viewing with an SEM. Milling a hard material canresult in “terracing,” that is, the edge rolls off in a series ofterraces, rather than having a sharp vertical drop. FIG. 8 showsterracing caused by a hard layer. The terracing can cause curtainingartifacts and other artifacts to be formed below the terracing. Sample800 includes a layer of aluminum oxide 802 over a layer of aluminum 804,which is softer than the oxide. A platinum protective layer 806deposited over the aluminum oxide layer reduces the creation of millingartifacts, but the protective layer does not eliminate terracing. FIG. 8shows the terraced edge 810 produced by the ion beam on the hard oxidelayer. The terraced edge 810 of the oxide layer causes irregularities812, such as curtaining artifacts, to be produced on the layer, such asaluminum layer 804, below the terracing.

FIG. 9 shows a scanning electron beam image of a sample 902 similar tothat shown schematically in FIG. 8. A layer 904 of aluminum oxide sitsover a layer of aluminum 906. A protective layer 908 is deposited overthe oxide layer 904 to reduce the creation of artifacts. After thetrench was milled to expose the cross section shown, the ion beam wasscanned across the exposed face to mill a “cleaning cross section” usinga current of about 180 nA. A “cleaning cross section” is typically asuccession of advancing, serial line mills. The hard aluminum oxidelayer shows terracing artifacts, which are difficult to observe in theblack region in FIG. 9. The terracing in the hard oxide layer causescurtaining in the softer aluminum layer 906 below the aluminum oxide.Terracing and other uneven milling artifacts can also be produced inmany materials when using high beam currents, such as from a plasma ionsource.

Terraced artifacts can be difficult and time-consuming to prevent usingprior art methods for reducing artifacts. Such methods include usingreduced milling current and high beam overlap between scans in the finalcleaning cross section. Some artifacts created when milling large crosssections are reduced by “rocking” the work piece, that is, alternatingthe ion beam impact angle, such as alternating the beam angle betweenplus 10 degrees and minus 10 degrees. Rocking does not reduce terracingartifacts, however. Terracing tends to create severe artifacts, such assevere curtaining, in the region below the terracing.

The most effective and widely proven alternative, backside milling,works reasonably well for TEM samples having a thickness of 50 to 100nm, but for ultra-thin samples having a sample thickness of 30 nm orless, even samples prepared by backside milling often show millingartifacts resulting in an undesirably non-uniform sample face. Further,even for thicker samples, backside milling requires a liftout andinversion operation that is very time consuming. Current backsidemilling techniques are also performed manually, and are unsuitable forautomation.

Thus, there is still a need for an improved method for the preparationof ultra-thin TEM samples that can reduce or eliminate bending andcurtaining, and that is suitable for an automated sample preparationprocess.

SUMMARY OF THE INVENTION

An object of the invention to prepare a sample by ion beam milling whileproducing little or no milling artifacts.

In some embodiments, the ion beam mills a trench to expose a crosssection for viewing with a scanning electron microscope. In otherembodiments, a lamella is produced for viewing on a TEM.

In embodiments for exposing an artifact-free cross section, after aninitial milling operation to produce a trench, a material is depositedon the face of the trench. The face is then milled to remove thedeposited material and produce an artifact-free surface.

In embodiments for producing a TEM sample, TEM lamellae less than 60nanometers thick, more preferably 30 nm or less in thickness, areproduced in a manner that reduces or prevents bending and curtaining.Some embodiments deposit material onto the face of a TEM sample duringthe process of preparing the sample. In some embodiments, the materialcan be deposited on a sample face that has already been thinned beforethe opposite face is thinned, which can serve to reinforce thestructural integrity of the sample and refill areas that have beenover-thinned due to the curtaining phenomena.

In some embodiments, such as when milling a cross section having layersof materials having different hardnesses, a cross section is exposed byion beam milling and then material is deposited onto the cross sectionface before a final milling of the cross section face, which depositioncan serve to reduce or eliminate curtaining on the sample face. In someembodiments, a deposition gas is provided while the ion beam is millingthe cross section, and in some embodiments, the deposition gas isprovided during a deposit step before the final milling of the crosssection.

It is noted that dissociation of the precursor can be achieved byexposing the sample (work piece) to energetic electrons, energetic ions,X-rays, light, heat, microwave radiation, or energizing the precursor inany other way, as a result of which the precursor material dissociatesin a non-volatile part that forms the deposit and a volatile part. Usingother energizing means than ion beams, for example using light producedby a laser, might offer advantages when filling irregularities or voidsprior to milling. Preferably the precursor is a good electric conductor,for example showing a conductivity of better than 100 μΩ·cm. Whendepositing occurs simultaneous with milling it makes more sense to usethe energetic ion beam to form a deposit.

The foregoing has outlined rather broadly the features and technicaladvantages of the present invention in order that the detaileddescription of the invention that follows may be better understood.Additional features and advantages of the invention will be describedhereinafter. It should be appreciated by those skilled in the art thatthe conception and specific embodiments disclosed may be readilyutilized as a basis for modifying or designing other structures forcarrying out the same purposes of the present invention. It should alsobe realized by those skilled in the art that such equivalentconstructions do not depart from the spirit and scope of the inventionas set forth in the appended claims.

It is noted that not only the preparation of thin samples, lamellae, isknown, but also the preparation of non-flat samples is known, forexample from U.S. Pat. No. 7,442,924B2. In U.S. Pat. No. 7,442,924B2 thesample being formed is roughly circular symmetric, i.e. in the form of acylinder or cone.

It is further noted that a sample can be a porous sample (the samplematerial containing voids). This is for example often the case wheninspecting catalysts.

In some embodiments directing an ion beam toward the work piece toremove material includes removing at least some deposited materials andsome sample material from the exposed surface to produce a smoothsurface.

BRIEF DESCRIPTION OF THE DRAWINGS

For a more thorough understanding of the present invention, andadvantages thereof, reference is now made to the following descriptionstaken in conjunction with the accompanying drawings, in which:

FIG. 1A shows the bulk milling process for preparing a TEM sample from abulk substrate according to the prior art.

FIG. 1B is a photomicrograph of a thinned TEM sample according to theprior art.

FIG. 2 is a photomicrograph of a thinned TEM sample showing curtainingon one sample face.

FIG. 3 is a flowchart showing the steps of creating a TEM sampleaccording to a preferred embodiment of the present invention.

FIG. 4 is a schematic representation showing the location of a sample tobe extracted within a larger bulk substrate.

FIGS. 5A-5I illustrate steps in carrying out the method of FIG. 3.

FIG. 6 shows a graph of ion current density versus position along aradial axis for a gallium focused ion beam.

FIG. 7 depicts one embodiment of an exemplary dual beam SEM/FIB systemthat is equipped to carry out embodiments of the present invention.

FIG. 8 shows schematically a work piece milled in accordance with priorart methods and exhibiting terracing artifacts and curtaining artifacts.

FIG. 9 is a photomicrograph showing terracing artifacts and curtainingartifacts of a sample processed in accordance with prior art methods.

FIG. 10 is a flow chart showing the steps of an embodiment of thepresent invention.

FIGS. 11A-11D show schematically a work piece at different stages ofprocessing according to an embodiment of the invention.

FIG. 12 is a photomicrograph showing a work piece processed inaccordance with an embodiment of the invention, the image being free ofcurtaining artifacts.

DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS

FIG. 10 is a flowchart showing the steps of an embodiment of theinvention. FIGS. 11A-11D shows the sample at different stages ofprocessing. FIG. 11A shows the sample 1102 includes a layer of aluminumoxide 1104 above a layer of aluminum 1106. In step 1002, a region ofinterest on the sample is identified. In step 1004, a protective layer1110 is deposited onto the surface of the sample 1104 over the region ofinterest. The protective layer can be deposited, for example, using ionbeam-induced deposition, electron beam-induced deposition, or otherlocal deposition process. Deposition precursors are well known and caninclude for example, metalloorganic compounds, such as tungstenhexacarbonyl and methylcyclopentadienlylplatinum (IV) trimethyl fordepositing metals, or hexamethylcyclohexasiloxane for depositing aninsulator.

In step 1006, a trench 1112 is milled in the sample to expose a crosssection 1114 as shown in FIG. 11A. The ion beam 1116 is typicallyoriented normal to the top surface of the sample when milling thetrench. The trench can be milled in part using a relatively large beamcurrent, “bulk mill” process, to cut the trench quickly. For example,when a gallium liquid metal ion source is used, a large current would begreater than about 5 nA, more preferably greater than about 10 nA andeven more preferably greater than about 20 nA. When using a FIB from aplasma ion source, a current of between about 50 nA and 2 μA could beused. In one embodiment, a beam of xenon ions from a plasma ion sourceis used. In another embodiment, a beam of gallium ions from a galliumliquid metal ion source is used. Milling the trench with a large beamcurrent can produce an uneven surface. After the large bulk mill processforms the trench, the exposed face 1114 is optionally milled using alower current to perform a “cleaning cross section” to smooth thesurface and remove grosser artifacts. The cleaning cross section sperformed using a beam current less than the beam current used for thebulk milling. FIG. 11B shows terracing artifact 1120 and exaggeratedirregularities 1122 that represent curtaining artifacts. The sample 1102at this point is similar to the prior art sample shown in FIG. 8 and/orFIG. 9.

After the trench is milled, the sample is tilted, typically to about 45degrees (from normal to the ion beam), in step 1008 as shown in FIG. 11Cto expose the milled face 1114 to the ion beam. In step 1010, aprecursor gas is provided at the sample surface in the region of trench1112 while the beam 1117 is directed to the sample to deposit a material1124 such as platinum onto face 1114 and onto part of the existingprotective layer 1110. The deposited material smooths both the terracedregion 1120 and the artifact-laden region 1122 below the terraced regionby at least partially filling in the terracing, the depressions andother irregularities to produce a smoother face. The deposited materialpartly planarizes the surface with the deposited material. The depositedmaterial preferably has a sputter rate similar to that of the underlyingmaterials. The deposited material can be a conductor or an insulator.Platinum has been found to be a suitable material to be deposited instep 1010.

In step 1012, the sample 1102 is tilted back to the original orientationas shown in FIG. 11D so that the beam sample surface is oriented normalto the ion beam. In step 1014, an ion beam 1118 is directed for a“cleaning cross section” at a lower current that the current used instep 1006. The beam removed the deposited material and theirregularities to produce a smooth face 1128 for observation. In someembodiments, the milling is stopped when all the deposited material isremoved. The end point can be determined by observing a charged particlebeam image of the face 1144, by analyzing, such as by secondary ion massspectroscopy, the material being milled, or by simply estimated the timerequired to remove the known thickness of the deposited material. Forexample, using a gallium liquid metal ion beam, the current for thecleaning cross section is typically between 0.1 nA and 4 nA. Using aplasma ion source, the cleaning cross section current is typicallybetween 15 nA and 180 nA. Step 1014 produces an artifact free surface.

FIG. 12 is a photomicrograph showing the results of an embodiment of theinvention. Comparing FIG. 12 with FIG. 9, one can see the absence of thecurtaining artifact in FIG. 12.

While the example described above formed a cross section of aluminumoxide over aluminum, the invention is applicable to a wide variety ofmaterials. It is particularly useful in layered structures in which onelayer is composed of a hard material, and for large cross-sections wherelarge beam currents are used. Applicants have demonstrated that theprocess produces artifact-free cross sections of other materials, suchas a cross section of carbon fibers in epoxy.

Although the described procedure includes an extra deposition step,embodiments of the invention can take less time to form a cross sectionthan the prior art by reducing total milling time.

Embodiments of the invention can improve the delineation of interfacesbetween layers of materials that are otherwise difficult to distinguishin an SEM image. For example, the boundary between a layer of a siliconoxide and a layer of a silicon nitride can be difficult to observe in anSEM image, making it impossible to accurately determine layer thicknessand uniformity. In some embodiments, a deposition precursor gas isprovided at the work piece surface while the surface is being etched toexpose a cross section for observation. This can result in a smoothercross section that exhibits improved contrast between the layers. Thebeam current is preferably sufficiently high to prevent a build up ofthe deposited material on the sample surface. The material is preferablyonly deposited in indentations that are constantly formed, filled andremoved by milling so that the milling operation continuously operateson a smooth, stable surface and there is little or no deposited materialleft on the surface when milling is complete.

In one embodiment, a bulk mill is performed to produce a trench with atriangular cross section to provide a wall normal to the sample surface.A “line mill” is then performed to produce a smooth wall. In someembodiments, the bulk mill process is performed without a depositionprecursor gas, and then the line mill process is performed whileproviding a deposition precursor gas at the sample surface near the beamimpact point. In other embodiments, the deposition precursor gas isprovided at the sample surface the entire time that the cross section isbeing milled, in both the bulk mill and the line mill.

The use of a deposition precursor while etching is also useful forproducing a smooth surface when milling materials having vias or otherair gaps, or having layers of materials of different densities. Priorart milled cross sections of such samples tend to be uneven. Using adeposition gas with the ion beam fills the voids and deposits materialinto the crevices left as the low density materials etch faster than thehigh density materials.

It is thought that the precursor decomposition reaction involves latticevibrations or secondary electrons and so is not limited to the exactpoint at which the ion beam impacts the work piece. This can allowprecursor decomposition in indentations that are not directly impactedby ions. In regions that are sufficiently close to the ion beam impactto dissociate the precursor molecule but not directly impacted orimpacted by fewer ions, the deposition reaction can outcompete thesputtering reaction to fill in the indentations.

When using a deposition precursor with a focused ion beam, it is knownthat, after a certain point, the deposition rate decreases as the beamcurrent increases because the ion beam sputters material faster than gasmolecules replenish on the surface to deposit material. The depositionand sputtering are competing processes in which the deposition islimited by the rate at which the deposition precursor diffuses to thesurface. Typical embodiments for producing a smooth cross section use acurrent of between 80 pA and 1 nA. While a beam energy of 30 keV istypical, a lower beam energy may be useful in some embodiments to reducesputtering and thereby increase deposition.

Some embodiments address problems of bending and curtaining during TEMsample preparation by adding material to the sample during the processof preparing the sample. In contrast to prior art methods which focusexclusively on removing material from the sample, preferred embodimentsof the present invention actually deposit additional material back ontothe sample during sample preparation.

In some preferred embodiments, as described in greater detail below, amaterial can be deposited onto a first TEM sample face after the firstface has been thinned, but before the second face is thinned. In someembodiments, all of the deposited material can be left on the thinnedfirst sample face while the second sample face is thinned. In otherembodiments, most of the deposited material can be removed from thefirst thinned side before the second side is thinned. The depositedmaterial left behind can serve to fill in the areas over-thinned bycurtaining effects. In either case, the presence of deposited materialon the sample face opposite the face being FIB milled can serve toreinforce the structural integrity of the sample.

In some preferred embodiments, material can be deposited onto the sampleface as it being thinned. As described above, undesirable curtainingeffects often result when a sample is composed of a mixture of morerapidly milling and slower milling materials. Applicants have discoveredthat by conducting the milling process in the presence of a suitableprecursor gas, material can be simultaneously deposited on some parts ofthe sample surface while other parts of the surface are being milledaway. The deposition gas is thought to decompose to fill indentationscreated by uneven milling rates, such as different etch rates ofdifferent materials. By continuously filling holes or other indentationsas they are being created by milling, the resulting cross section issmoother and exhibits less distortion than would be produced otherwise,to provide a better representation of the actual structure. In otherembodiments, the sample face can be coated after a fraction of the FIBthinning has been performed on the face. By either or both of thesemethods, the areas of the sample face having a higher milling rate canbe protected or even re-filled by deposited material during the thinningprocess, thus reducing or preventing curtaining of the sample face.

According to preferred embodiments of the present invention, some or allof the deposited material is removed before sample imaging; in otherembodiments the material deposited is sufficiently electron transparentat the desired imaging parameters that it can be left in place duringsample TEM analysis. Where some or all of the deposited material is tobe removed, any known suitable method can be used for material removal.As will be recognized by persons of skill in the art, a suitablematerial removal method will depend upon a number of factors such as thematerial deposited and the structural integrity of the sample.Preferably, the selected material removal method will selectively removethe deposited material causing little if any additional sample materialremoval from the TEM sample.

It should be noted that the embodiments described above can be usedtogether, separately, or in any desired combination. For example, insome embodiments material will only be deposited onto a sample faceafter it has been thinned, while in other embodiments material can bedeposited both during thinning and after thinning a sample face. Apreferred method or apparatus of the present invention has many novelaspects, and because the invention can be embodied in different methodsor apparatuses for different purposes, not every aspect need be presentin every embodiment. Moreover, many of the aspects of the describedembodiments may be separately patentable.

FIG. 3 is a flowchart showing the steps of creating a TEM sampleaccording to a preferred embodiment of the present invention. First, instep 301, a substrate such as a semiconductor wafer, a frozen biologicalmaterial, or a mineral sample is loaded into a suitable processing toolsuch as a Dual Beam FIB/SEM system having both a FIB column and a SEMcolumn. One such suitable beam FIB/SEM system is the Helios1200 or theExpida™ 1255 DualBeam™ System, available from FEI Company of Hillsboro,Oreg., the assignee of the present invention.

Referring also to FIG. 7, the typical dual-beam system 702 configurationis an electron column 704 having a vertical axis with an ion column 706having an axis tilted with respect to the vertical (usually at a tilt ofapproximately 52 degrees). Wafers are preferably transferred by way of amulti-wafer carrier and auto-loading robot (not shown), as is well knownin the art, although wafers can also be transferred manually.

In step 302, the location of a TEM sample (containing a feature ofinterest) to be extracted from a substrate is determined. For example,the substrate may be a silicon semiconductor wafer or portion thereofand the portion to be extracted may include a portion of an integratedcircuit formed on the silicon wafer that is to be observed using theTEM. In other example, the substrate could be an AlTiC wafer and theextracted portion might include a structure used for reading or writingdata onto a storage medium. In other example, the substrate could be asample containing a natural resource and extraction might be performedto analyze characteristics of the resource in the sample. FIG. 4 is aschematic representation showing the location of the sample 102 to beextracted within a larger substrate 108.

In step 304, the substrate is preferably oriented so that its topsurface is perpendicular to a focused ion beam emitted from the FIBcolumn 706. A focused ion beam using a high beam current with acorrespondingly large beam size is then used to mill large amounts ofmaterial away from the front and back portion of a sample sectioncontaining the desired TEM sample in step 306. Bulk material removal ispreferably performed at high beam current, preferably at highestcontrollable current available in order remove the bulk material as fastas possible. For example, bulk material removal could be performed usinga 13 nA gallium ion beam with a 30 kV accelerating voltage. In somecircumstances it may be desirable to mill the substrate with the TEMsample oriented at an acute angle relative to the substrate surface. Forexample, U.S. Pat. No. 6,039,000 to Libby et al, for Focused ParticleBeam Systems and Methods Using a Tilt Column (2000), which is assignedto the assignee of the present invention and hereby incorporated byreference, describes creating a TEM sample using a FIB oriented at anangle relative to the sample surface by etching a cavity on either sideof desired TEM sample.

As in the prior art method shown in FIG. 1, once the bulk milling iscompleted, the remaining material between the two milled rectangles 14and 15 forms a vertical sample section 102, which is still attached tothe bulk substrate at the sides and base. FIG. 5A shows such a verticalsample section 102, although none of the surrounding bulk substrate isshown for clarity.

After bulk thinning, in step 308, the sample section 102 is then furtherthinned on a first side 51A (preferably using progressively finer beamsizes and lower beam energy) until the desired first sample face isreached. For example, the first phase of thinning might use a beamcurrent of 1 nA ion beam, followed by a second phase using a 100 pAbeam. As illustrated in FIG. 5B, the exposed first sample face willtypically display some degree of curtaining, resulting in over-milledareas 52. The sample is preferably thinned using an ion beam with anaxis oriented normal or perpendicular to the top surface of the sample,although a non-normal angle could also be used if the beam axis isoriented to the side of the desired TEM sample face.

The differences in material thickness shown in FIG. 5B is only forillustration purposes and not intended to show exact scale of differencein thickness between the working surface and the troughs caused bycurtaining or to indicate that the surface variations will necessarilybe uniform. The arrows indicating the FIB 706 and SEM beam 704 or otherprocesses shown schematically in FIGS. 5B-5I are only intended toillustrate the process being applied, not the angle or orientation ofthe beams or the exact location of the deposition or etching.

In step 310, once the desired sample face has been exposed, material 56is deposited onto the exposed sample face. Preferably, a layer ofmaterial 56 is deposited onto the entire sample face, for example, byusing a precursor gas 54 and chemical vapor deposition, using either theion beam or an electron beam (depending in part upon the material beingdeposited). The mechanism for activating the precursors could be SEM,FIB, indirect delivery of secondary particles, or other techniques.Further, the deposition technique is not limited to beam activatedprecursor deposition.

The material deposited preferably has a different composition than theTEM sample material(s). The choice of material to be deposited maydepend upon the particular application of the TEM sample. Suitabledeposited materials may include, for example, tungsten, platinum, gold,carbon, silicon oxides, or any other suitable materials. Precursor gasesfor depositing these materials are well known in the prior art.

Also, as discussed in greater detail below, the deposited materialeither will be removed during the thinning process or will be easilyremovable after the critical milling of the TEM sample is completed. Forexample, where the deposition material is carbon, which can be depositedby carbon vapor deposition, the deposition material can be removedthrough water vapor etching, which is a very selective etching processthat will not cause additional damage to the non-carbon TEM sample. Insome preferred embodiments, the deposited material may be one which willnot significantly interfere with imaging the TEM sample, in which caseit can be left in place. For instance, in applications involvingchemical analysis of the sample, the known compounds present indeposited material can be ignored.

In the embodiment shown in FIG. 5C, material 56 is added so that theoverall thickness of the original sample section 102 is increased. Inother words, more material is added than was removed during the thinningprocess. This amount of additional material is not required, however, aslong as the added material is sufficient to adequately increase thestructural integrity of the sample or to fill in a sufficient amount ofthe curtaining over-milling. The thickness of the deposited layer ofthickness depends on how much beam exposure is expected and whatmaterial is being deposited. For example, if a Carbon-based material isdeposited mainly for the purpose of structural integrity and it willreceive minimal erosion from beam exposure, then a deposition layer ofapproximately 20 nm might be appropriate. If the layer is being used toreduce curtaining during a 1 nA milling step, then a thickness of 100 nmor more might be deposited.

In step 312, a portion of the added material 56 is optionally removed.Because the deposited material is composed of a single compound, littleor no curtaining will result as the material is removed. Preferablyenough deposited material 56 is left on the sample face 51A to provideadditional structural integrity as the other sample face 51B is milled,although all of the deposited material could be removed beforeproceeding to the second sample face in situations where sample bendingis a low priority and the only real concern is the reduction incurtaining. As discussed below, in some preferred embodiments, materialcan be deposited onto the sample before the final sample face isexposed. The deposited material could then be removed during subsequentadditional thinning. The steps of thinning, adding material, andthinning again could be repeated iteratively until the final sample faceis exposed. This iterative technique can be useful in minimizing thecurtaining effect or if it is desirable can be employed as anend-pointing technique of the thinning step.

Then, in step 314, the FIB is directed at the second TEM sample face 51B(backside) of sample 102 to thin the sample. Again, progressively finerbeam sizes and lower beam energies are used to expose the desired sampleface. For example, the first phase of thinning might use a beam currentof 1 nA ion beam, followed by a second phase using a 100 pA beam. Asillustrated in FIG. 5F, the exposed second sample face 51B willtypically also display some degree of curtaining, resulting inover-milled areas 52.

In step 316, material 56 is also deposited onto the second sample face51B using a suitable process such as chemical vapor deposition. In step318, some or all of the deposited material on the second face isremoved, for example by FIB milling. The material deposited on thebackside would also be added and removed iteratively in multiple steps,with all of the material removed on the final thinning step.

Optionally, in step 320, all of the deposited material 56 can be removedfrom the completed TEM sample 110. The material removal can beaccomplished via FIB milling, or by a method that will be lessdestructive to the TEM sample material such as a selective gas-assistedetching, either with the ion beam or with an electron beam. In otherpreferred embodiments, the deposited material can be etched away in, forexample, an acid bath after the TEM sample is removed from the vacuumchamber. The present invention is not limited to these examples, and anysuitable type of beam-based removal or chemistry removal, or plasmainduced removal may be utilized. If there are other samples to beextracted from the substrate (step 322) the process returns to step 302and the next sample site is located. If not, in step 324 the processstops.

In some preferred embodiments of the present invention, material canalso be deposited onto the TEM sample face during the thinning process.According to some preferred embodiments, two charged particle beamscould be used at one time. For example, in a dual beam system such asthe one shown in FIG. 7 below, the electron beam could be used with asuitable precursor gas to deposit the material onto the sample face,while the FIB could be used for milling.

In other embodiments, an ion beam could be used to deposit and removematerial at the same time. A focused ion beam system typically has acircularly symmetric, substantially Gaussian current densitydistribution, as illustrated in FIG. 6, which shows a graph of ioncurrent density versus position along a radial axis. As shown in FIG. 6,the current density at the center of the beam is highest (and thus millsfaster) while the beam current tapers off away from the center of thebeam.

This beam current spread is one of the main contributors to curtaining.As the beam is milling the lamella face with the center of the beam, theions in the tail of the Gaussian distribution are reaching samplematerial in advance of (and behind) the center of the beam. The lowercurrent portion of the beam may have little effect upon the heaviermetal sample structures having low milling rates; however, the lightermaterials with higher milling rates may be milled to a significantdegree.

Applicants have discovered that this “advance” milling can be reduced oreliminated by directing a suitable precursor gas toward the samplesurface in the presence of the beam. As is well known in the prior art,when the charged particle beam irradiates the substrate with theadsorbed layer of precursor gas, secondary electrons are emitted fromthe substrate. These secondary electrons cause a dissociation of theadsorbed precursor gas molecules. Part of the dissociated precursormaterial forms a deposit on the substrate surface, while the rest of theprecursor gas particle forms a volatile by-product and is pumped away bythe vacuum system of the apparatus.

In the presence of a suitable precursor gas, the outlying lower currentportions of the beam can provide secondary electrons to cause depositionof the dissociated precursor material. This deposited material must thenbe sputtered away before the underlying substrate is milled. Preferably,the beam current in the center of the beam is high enough to switch thedominant reaction from deposition to milling. In this fashion, thedeposited material can serve as a protective layer to preventsignificant milling of the lighter, higher milling rate material inadvance of the center of the beam, while the center of the beam millsaway both the newly deposited protective layer and the underlyingsubstrate at roughly the same rate. Because the beam current is lower atthe outlying edges of the beam, the lighter material covered by aprotective layer will not etch significantly and curtaining will beprevented or at least substantially reduced. Skilled persons will beable to select a suitable precursor gas and adjust the gas pressure andbeam current so that the predominant reaction is deposition at theoutlying lower current portions of the beam and etching (milling) at thecenter of the beam.

In some preferred embodiments, the rate of deposition may be higher thanthe rate of etching even for the center of the beam so that a protectivelayer is deposited on the entire surface. The beam parameters or gaspressures can then be adjusted so that etching predominates, either forthe entire beam or only for the center high current portion of the beam.Further, according to some embodiments, once some degree of curtainingbegins to form during sample milling, the voids in the sample face wherethe lighter material has been over-milled will tend to have a curvedbowl-like shape. Because of the curvature of the walls of the bowls,precursor material will tend to deposit in these regions at a higherrate than on the rest of the sample face. As a result, the beamparameters and precursor gas pressures can be adjusted so that thedeposited material will tend to fill in the low areas, thus filling inthe curtaining to some degree and protecting the low areas from furtherover-milling.

Embodiments of the present invention thus provide a means of reducing orpreventing sample bending (along with other types of stress-based sampledamage) and/or curtaining on the sample face. This is particularlyimportant for ultra-thin samples (defined herein as samples having athickness of 30 nm or less). Applicants have confirmed experimentallythat the deposition of a suitable layer of deposited material on onesample face will allow a silicon TEM sample to be thinned toapproximately 30 nm without bending, when similar samples withoutdeposited material had significant bending long before a 30 nm thicknesswas reached.

Depending upon the particular sample type, it may be more important toavoid one or the other of these types of sample damage. For example, ina sample where the entire structure of interest is less than 100 nmwide, but it sits directly underneath a vertical boundary between a fastmilling and slow milling material, curtaining would be the critical typeof damage, while sample bending might be irrelevant. In such cases whereonly one type of damage is important, it may not be necessary to use allof the steps in the method described above. Also, the depositionmaterial does not need to be applied to both faces of a sample. Forexample, when preparing samples for which bending is the primaryconcern, it may be sufficient to deposit material only on the firstsample face after it is thinned, and then to remove that depositedmaterial after the second sample face is exposed. In some embodiments,the steps of depositing material onto the sample face, and thinning thesample face, then depositing more material onto the sample face may beconducted iteratively until the desired sample thickness has beenreached.

The improved structural integrity of the sample being thinned also makesthe method of TEM sample production according to the present inventionmore suited for automated handling and processing, which increases easeof use and can lower cost per sample for our customers. The reduction ofcurtaining effects allows production of high quality samples withshorter site times and/or greater ease of use than prior artsilicon-side milling techniques.

The steps described above can also be applied in any desired order. Forexample, in some situations it might be desirable to deposit materialbefore any thinning takes place. The sample can also be imaged at anypoint during the process. Also for example, the deposition of materialon the sample face might not be initiated until the sample has beensufficiently thinned and imaging has been performed to recognize thedesired features within the sample that will be the targets for thefinal TEM sample faces. In some preferred embodiments, the materialdeposition and material removal actions are distinct serial steps. Inother embodiments, the deposition and material removal processes can becarried out simultaneously, either on the same face or on differentfaces, during at least part of the sample preparation.

FIG. 7 depicts one embodiment of an exemplary dual beam SEM/FIB system702 that is equipped to carry out embodiments of the present invention.Embodiments of the present invention can be used in a wide variety ofapplications where a low resistivity material is deposited onto a targetsurface of a substrate. Preparation and analysis of such a sample istypically performed in a dual beam electron beam/focused ion beam systemsuch as the one now described. Suitable dual beam systems arecommercially available, for example, from FEI Company, Hillsboro, Oreg.,the assignee of the present application. While an example of suitablehardware is provided below, the invention is not limited to beingimplemented in any particular type of hardware.

Dual beam system 702 has a vertically mounted electron beam column 704and a focused ion beam (FIB) column 706 mounted at an angle ofapproximately 52 degrees from the vertical on an evacuable specimenchamber 708. The specimen chamber may be evacuated by pump system 709,which typically includes one or more, or a combination of, aturbo-molecular pump, oil diffusion pumps, ion getter pumps, scrollpumps, or other known pumping means.

The electron beam column 704 includes an electron source 710, such as aSchottky emitter or a cold field emitter, for producing electrons, andelectron-optical lenses 712 and 714 forming a finely focused beam ofelectrons 716. Electron source 710 is typically maintained at anelectrical potential of between 500 V and 30 kV above the electricalpotential of a work piece 718, which is typically maintained at groundpotential.

Thus, electrons impact the work piece 718 at landing energies ofapproximately 500 eV to 30 keV. A negative electrical potential can beapplied to the work piece to reduce the landing energy of the electrons,which reduces the interaction volume of the electrons with the workpiece surface, thereby reducing the size of the nucleation site. Workpiece 718 may comprise, for example, a semiconductor device,microelectromechanical system (MEMS), data storage device, or a sampleof material being analyzed for its material characteristics orcomposition. The impact point of the beam of electrons 716 can bepositioned on and scanned over the surface of a work piece 718 by meansof deflection coils 720. Operation of lenses 712 and 714 and deflectioncoils 720 is controlled by scanning electron microscope power supply andcontrol unit 722. Lenses and deflection unit may use electric fields,magnetic fields, or a combination thereof.

Work piece 718 is on movable stage 724 within specimen chamber 708.Stage 724 can preferably move in a horizontal plane (X-axis and Y-axis)and vertically (Z-axis) and can tilt approximately sixty (60) degreesand rotate about the Z-axis. A door 727 can be opened for inserting workpiece 718 onto X-Y-Z stage 724 and also for servicing an internal gassupply reservoir (not shown), if one is used. The door is interlocked sothat it cannot be opened if specimen chamber 708 is evacuated.

Mounted on the vacuum chamber are one or more gas injection systems(GIS) 730. Each GIS may comprise a reservoir (not shown) for holding theprecursor or activation materials and a needle 732 for directing the gasto the surface of the work piece. Each GIS further comprises means 734for regulating the supply of precursor material to the work piece. Inthis example the regulating means are depicted as an adjustable valve,but the regulating means could also comprise, for example, a regulatedheater for heating the precursor material to control its vapor pressure.

When the electrons in the electron beam 716 strike work piece 718,secondary electrons, backscattered electrons, and Auger electrons areemitted and can be detected to form an image or to determine informationabout the work piece. Secondary electrons, for example, are detected bysecondary electron detector 736, such as an Everhart-Thornley detector,or a semiconductor detector device capable of detecting low energyelectrons. STEM detector 762, located beneath the TEM sample holder 761and the stage 724, can collect electrons that are transmitted through asample mounted on the TEM sample holder. Signals from the detectors 736,762 are provided to a system controller 738. Said controller 738 alsocontrols the deflector signals, lenses, electron source, GIS, stage andpump, and other items of the instrument. Monitor 740 is used to displayuser controls and an image of the work piece using the signal

The chamber 708 is evacuated by pump system 709 under the control ofvacuum controller 741. The vacuum system provides within chamber 708 avacuum of approximately 7×10-6 mbar. When a suitable precursor oractivator gas is introduced onto the sample surface, the chamberbackground pressure may rise, typically to about 5×10-5 mbar.

Focused ion beam column 706 comprises an upper neck portion 744 withinwhich are located an ion source 746 and a focusing column 748 includingextractor electrode 750 and an electrostatic optical system including anobjective lens 751. Ion source 746 may comprise a liquid metal galliumion source, a plasma ion source, a liquid metal alloy source, or anyother type of ion source. The axis of focusing column 748 is tilted 52degrees from the axis of the electron column. An ion beam 752 passesfrom ion source 746 through focusing column 748 and betweenelectrostatic deflectors 754 toward work piece 718.

FIB power supply and control unit 756 provides an electrical potentialat ion source 746. Ion source 746 is typically maintained at anelectrical potential of between 1 kV and 60 kV above the electricalpotential of the work piece, which is typically maintained at groundpotential. Thus, ions impact the work piece at landing energies ofapproximately 1 keV to 60 keV. FIB power supply and control unit 756 iscoupled to deflection plates 754 which can cause the ion beam to traceout a corresponding pattern on the upper surface of work piece 718. Insome systems, the deflection plates are placed before the final lens, asis well known in the art. Beam blanking electrodes (not shown) withinion beam focusing column 748 cause ion beam 752 to impact onto blankingaperture (not shown) instead of work piece 718 when a FIB power supplyand control unit 756 applies a blanking voltage to the blankingelectrode.

The ion source 746 typically provides a beam of singly charged positivegallium ions that can be focused into a sub one-tenth micrometer widebeam at work piece 718 for modifying the work piece 718 by ion milling,enhanced etch, material deposition, or for imaging the work piece 718.

A micromanipulator 757, such as the AutoProbe 200™ from Omniprobe, Inc.,Dallas, Tex., or the Model MM3A from Kleindiek Nanotechnik, Reutlingen,Germany, can precisely move objects within the vacuum chamber.Micromanipulator 757 may comprise precision electric motors 758positioned outside the vacuum chamber to provide X, Y, Z, and thetacontrol of a portion 759 positioned within the vacuum chamber. Themicromanipulator 757 can be fitted with different end effectors formanipulating small objects. In the embodiments described herein, the endeffector is a thin probe 760. As is known in the prior art, amicromanipulator (or microprobe) can be used to transfer a TEM sample(which has been freed from a substrate, typically by an ion beam) to aTEM sample holder 761 for analysis.

System controller 738 controls the operations of the various parts ofdual beam system 702. Through system controller 738, a user can causeion beam 752 or electron beam 716 to be scanned in a desired mannerthrough commands entered into a conventional user interface (not shown).Alternatively, system controller 738 may control dual beam system 702 inaccordance with programmed instructions. FIG. 7 is a schematicrepresentation, which does not include all the elements of a typicaldual beam system and which does not reflect the actual appearance andsize of, or the relationship between, all the elements.

Although the description of the present invention above is mainlydirected at methods of preparing ultra-thin TEM samples, it should berecognized that an apparatus performing the operation of such a methodwould further be within the scope of the present invention. Further, itshould be recognized that embodiments of the present invention can beimplemented via computer hardware, a combination of both hardware andsoftware, or by computer instructions stored in a non-transitorycomputer-readable memory. The methods can be implemented in computerprograms using standard programming techniques—including anon-transitory computer-readable storage medium configured with acomputer program, where the storage medium so configured causes acomputer to operate in a specific and predefined manner—according to themethods and figures described in this Specification. Each program may beimplemented in a high level procedural or object oriented programminglanguage to communicate with a computer system. However, the programscan be implemented in assembly or machine language, if desired. In anycase, the language can be a compiled or interpreted language. Moreover,the program can run on dedicated integrated circuits programmed for thatpurpose.

Further, methodologies may be implemented in any type of computingplatform, including but not limited to, personal computers,mini-computers, main-frames, workstations, networked or distributedcomputing environments, computer platforms separate, integral to, or incommunication with charged particle tools or other imaging devices, andthe like. Aspects of the present invention may be implemented in machinereadable code stored on a storage medium or device, whether removable orintegral to the computing platform, such as a hard disc, optical readand/or write storage mediums, RAM, ROM, and the like, so that it isreadable by a programmable computer, for configuring and operating thecomputer when the storage media or device is read by the computer toperform the procedures described herein. Moreover, machine-readablecode, or portions thereof, may be transmitted over a wired or wirelessnetwork. The invention described herein includes these and other varioustypes of computer-readable storage media when such media containinstructions or programs for implementing the steps described above inconjunction with a microprocessor or other data processor. The inventionalso includes the computer itself when programmed according to themethods and techniques described herein.

Computer programs can be applied to input data to perform the functionsdescribed herein and thereby transform the input data to generate outputdata. The output information is applied to one or more output devicessuch as a display monitor. In preferred embodiments of the presentinvention, the transformed data represents physical and tangibleobjects, including producing a particular visual depiction of thephysical and tangible objects on a display.

Preferred embodiments of the present invention also make use of aparticle beam apparatus, such as a FIB or SEM, in order to image asample using a beam of particles. Such particles used to image a sampleinherently interact with the sample resulting in some degree of physicaltransformation. Further, throughout the present specification,discussions utilizing terms such as “calculating,” “determining,”“measuring,” “generating,” “detecting,” “forming,” or the like, alsorefer to the action and processes of a computer system, or similarelectronic device, that manipulates and transforms data represented asphysical quantities within the computer system into other data similarlyrepresented as physical quantities within the computer system or otherinformation storage, transmission or display devices.

The invention has broad applicability and can provide many benefits asdescribed and shown in the examples above. The embodiments will varygreatly depending upon the specific application, and not everyembodiment will provide all of the benefits and meet all of theobjectives that are achievable by the invention. Particle beam systemssuitable for carrying out the present invention are commerciallyavailable, for example, from FEI Company, the assignee of the presentapplication.

Although much of the previous description is directed at semiconductorwafers, the invention could be applied to any suitable substrate orsurface. Further, the present invention could be applied to samples thatare thinned in the vacuum chamber but removed from the substrate outsidethe vacuum chamber (ex-situ-type samples) or to samples extracted fromthe substrate and thinned after mounting on a TEM grid inside the vacuumchamber (in-situ-type samples). Whenever the terms “automatic,”“automated,” or similar terms are used herein, those terms will beunderstood to include manual initiation of the automatic or automatedprocess or step. In the following discussion and in the claims, theterms “including” and “comprising” are used in an open-ended fashion,and thus should be interpreted to mean “including, but not limited to .. . ” The term “integrated circuit” refers to a set of electroniccomponents and their interconnections (internal electrical circuitelements, collectively) that are patterned on the surface of amicrochip. The term “semiconductor device” refers generically to anintegrated circuit (IC), which may be integral to a semiconductor wafer,singulated from a wafer, or packaged for use on a circuit board. Theterm “FIB” or “focused ion beam” is used herein to refer to anycollimated ion beam, including a beam focused by ion optics and shapedion beams.

To the extent that any term is not specially defined in thisspecification, the intent is that the term is to be given its plain andordinary meaning. The accompanying drawings are intended to aid inunderstanding the present invention and, unless otherwise indicated, arenot drawn to scale.

The invention provides a method of preparing a sample for analysis, themethod comprising:

directing an ion beam toward a work piece to remove material and exposea surface, the exposed surface having irregularities;

depositing material on the exposed surface, the deposited materialsmoothing the irregularities;

directing an ion beam toward the work piece to remove the depositedmaterials and some material from the exposed surface to produce a smoothcross sectional face.

In some embodiments, the method further comprises depositing aprotective layer onto the surface of the work piece using chargedparticle beam deposition.

In some embodiments, directing an ion beam toward a work piece to removematerial includes directing an ion beam perpendicular to the work piecesurface.

In some embodiments, depositing material on the exposed surface includestilting the work piece and depositing the material using chargedparticle beam deposition.

In some embodiments, directing an ion beam toward a work piece to removematerial and expose a surface includes directing the ion beam using afirst beam current and directing an ion beam toward the work piece toremove the deposited materials includes directing the ion beam using asecond beam current, less than the first beam current.

In some embodiments, directing an ion beam toward a work piece to removematerial and expose a surface includes directing an ion beam from aplasma ion source, the ion beam having a beam current greater than 50nA.

In some embodiments, directing an ion beam toward a work piece to removematerial includes cutting a trench to expose a cross section forobservation by a scanning electron microscope.

In some embodiments, directing an ion beam toward a work piece to removematerial includes forming a lamella for observation on a transmissionelectron microscope.

In some embodiments, directing an ion beam toward a work piece includesdirecting an ion beam toward a work piece composed of layers ofmaterials of different hardnesses, the ion beam creating theirregularities in a softer layer after passing through harder layer.

In some embodiments, directing an ion beam toward a work piece includesdirecting an ion beam toward a work piece composed of at least a layerof a metal and a layer of an oxide or nitride of the metal.

In some embodiments, the method further comprises directing an ion beamtoward a work piece to expose a second face depositing a layer of amaterial onto the exposed second sample face.

In some embodiments, include a charged particle beam apparatuscomprising:

an ion source;

a focusing column for focusing the ions onto a work piece in a samplevacuum chamber;

a gas injection system for providing a precursor gas at the work piecesurface;

a controller for controlling the operation of the charged particle beamsystem in accordance with stored computer-readable instructions; and

a computer readable memory storing computer instruction for controllingthe charged particle beam system to:

directing an ion beam toward a work piece to remove material and exposea surface, the exposed surface having irregularities;

depositing material on the exposed surface, the deposited materialsmoothing the irregularities;

directing an ion beam toward the work piece to remove the depositedmaterials and some material from the exposed surface to produce a smoothcross sectional face.

Some embodiments comprise a non-transitory computer-readable storagemedium configured with a computer program, where the storage medium soconfigured causes a computer to control a charged particle beam systemto carry out the steps of the method described above.

Some embodiments provide a method of making producing a smooth surfaceby ion beam milling, comprising:

directing a focused ion beam toward a surface of a work piece to removematerial to expose an interior surface of the work piece; and

directing a deposition precursor gas toward the work piece whiledirecting the focused ion beam, the ion beam initiating decomposition ofthe precursor gas to deposit a material on the surface of the work piecewhile simultaneously milling material from the substrate to produce asmooth surface for viewing.

In some embodiments, the method further comprises forming an image ofthe wall using an electron beam.

In some embodiments, the wall is normal to the work piece surface.

In some embodiments, the wall is formed using a line mill.

In some embodiments, the method further comprises milling a trench inthe work piece without using a deposition gas and in which the wall isformed at the trench edge.

In some embodiments the sample material is a porous material.

In some embodiments the sample is a sample that is not a thin flatsample (is not a lamella).

Although the present invention and its advantages have been described indetail, it should be understood that various changes, substitutions andalterations can be made herein without departing from the spirit andscope of the invention as defined by the appended claims. Moreover, thepresent application is not intended to be limited to the particularembodiments of the process, machine, manufacture, composition of matter,means, methods and steps described in the specification. As one ofordinary skill in the art will readily appreciate from the disclosure ofthe present invention, processes, machines, manufacture, compositions ofmatter, means, methods, or steps, presently existing or later to bedeveloped that perform substantially the same function or achievesubstantially the same result as the corresponding embodiments describedherein may be utilized according to the present invention. Accordingly,the appended claims are intended to include such processes, machines,manufacture, compositions of matter, means, methods, or steps.

We claim as follows:
 1. A method of preparing a sample for analysis, themethod comprising: directing an ion beam toward a work piece to removematerial and expose a surface, the exposed surface havingirregularities; depositing material on the exposed surface, thedeposited material smoothing the irregularities; and directing an ionbeam toward the work piece to remove at least some deposited materialsand some material from the exposed surface to produce a smooth surface.2. The method of claim 1 in which the sample material is a porousmaterial.
 3. The method of claim 1 in which the deposited material isformed by the dissociation of a precursor material, and the precursormaterial is activated by exposing the exposed surface to electrons,ions, X-rays, light, heat, or microwave radiation, as a result of whichthe precursor material dissociates in a non-volatile part that forms thedeposit and a volatile part.
 4. The method of claim 1 further comprisingdepositing a protective layer onto the surface of the work piece usingcharged particle beam deposition.
 5. The method of claim 1 in whichdirecting an ion beam toward a work piece to remove material includesdirecting an ion beam perpendicular to the work piece surface.
 6. Themethod of claim 1 in which depositing material on the exposed surfaceincludes tilting the work piece and depositing the material usingcharged particle beam deposition.
 7. The method of claim 1 in whichdirecting an ion beam toward a work piece to remove material and exposea surface includes directing the ion beam using a first beam current andin which directing an ion beam toward the work piece to remove thedeposited materials includes directing the ion beam using a second beamcurrent, less than the first beam current.
 8. The method of claim 1 inwhich directing an ion beam toward a work piece to remove material andexpose a surface includes directing an ion beam from a plasma ionsource, the ion beam having a beam current greater than 50 nA.
 9. Themethod of claim 1 in which directing an ion beam toward a work piece toremove material includes cutting a trench to expose a cross section forobservation by a scanning electron microscope.
 10. The method of claim 1in which directing an ion beam toward a work piece to remove materialincludes forming a lamella for observation on a transmission electronmicroscope.
 11. The method of claim 1 in which directing an ion beamtoward a work piece includes directing an ion beam toward a work piececomposed of layers of materials of different hardnesses, the ion beamcreating the irregularities in a softer layer after passing throughharder layer.
 12. The method of claim 1 in which directing an ion beamtoward a work piece includes directing an ion beam toward a work piececomposed of at least a layer of a metal and a layer of an oxide ornitride of the metal.
 13. The method of claim 1 further comprisingdirecting an ion beam toward a work piece to expose a second facedepositing a layer of a material onto the exposed second sample face.14. An charged particle beam apparatus comprising: an ion source; afocusing column for focusing the ions onto a work piece in a samplevacuum chamber; a gas injection system for providing a precursor gas atthe work piece surface; a controller for controlling the operation ofthe charged particle beam system in accordance with storedcomputer-readable instructions; and a computer readable memory storingcomputer instruction for controlling the charged particle beam systemto: directing an ion beam toward a work piece to remove material andexpose a surface, the exposed surface having irregularities; depositingmaterial on the exposed surface, the deposited material smoothing theirregularities; directing an ion beam toward the work piece to removethe deposited materials and some material from the exposed surface toproduce a smooth cross sectional face.
 15. A non-transitorycomputer-readable storage medium configured with a computer program,where the storage medium so configured causes a computer to control acharged particle beam system to carry out the steps of the method ofclaim 1.